CN104080944A - Organosilane precursors for ALD/CVD silicon-containing film applications - Google Patents

Organosilane precursors for ALD/CVD silicon-containing film applications Download PDF

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CN104080944A
CN104080944A CN201380007437.1A CN201380007437A CN104080944A CN 104080944 A CN104080944 A CN 104080944A CN 201380007437 A CN201380007437 A CN 201380007437A CN 104080944 A CN104080944 A CN 104080944A
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precursor
film
alkyl
reactant
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CN104080944B (en
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C·迪萨拉
G·库肯拜泽尔
V·R·帕里姆
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • C23C16/24—Deposition of silicon only
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Abstract

Disclosed are Si-containing thin film forming precursors, methods of synthesizing the same, and methods of using the same to deposit silicon-containing films using vapor deposition processes for manufacturing semiconductors, photovoltaics, LCD-TFT, flat panel-type devices, refractory materials, or aeronautics.

Description

For the organosilane precursor of ALD/CVD silicon-containing film application
Quoting alternately of related application
The application advocates the U.S. Provisional Application the 61/674th of application on July 20th, 2012, the right of priority of No. 103, and the full content of this application is incorporated herein for reference.
Technical field
Openly form precursor, its synthetic method containing Si film and use it to use the method for vapour deposition process depositing silicon-containing films for the manufacture of semi-conductor, photovoltaic devices, LCD-TFT, plate device, refractory materials or aeronautical material.
Prior art
Be widely used in semi-conductor, photovoltaic devices, LCD-TFT, plate device, refractory materials or Aviation Industry containing Si film.Can be for example as the dielectric materials (SiO insulating with electrical properties containing Si film 2, SiN, SiCN, SiCOH, MSiOx, wherein M is that Hf, Zr, Ti, Nb, Ta or Ge and x are greater than zero), can be used as conductive film containing Si film, as metal silicide or metal silicon nitride.Because electrical devices framework reduces towards nano level (especially lower than 28nm node) strict demand that size applies, need the molecular precursor of more and more meticulous adjusting, these molecular precursor also meet volatility (for ALD processing procedure), lower process temperatures, and the reactivity of various oxygenants and the requirement of low Film Contamination except having the conformality of high deposition rate, the film that produces and firmness.
Know silane (SiH 4) can be used for hot CVD.But this molecule tool pyrophoricity, makes this room temperature air face the challenge aspect safe handling thus.Use and adopted halogenated silanes (as dichlorosilane SiH 2cl 2) CVD method.But these methods may need long purge time, cause the halogen of film to pollute and particle formation (by ammonium chloride salt formation), and even destroy some matrix, thereby cause that undesirable interfacial layer forms.With moieties substitute halogen and can obtain some and improve, but cost is to produce disadvantageous Prevent Carbon Contamination in film.
Organic amino base silane has been used as the precursor containing the CVD of Si film.The people's such as Dussarrat US7192626 has reported and has used three silanamines N (SiH 3) 3deposit SiN film.Other precursors of having reported comprise diisopropyl ammonia base silane [SiH 3(NiPr 2)] and similar SiH 3(NR 2) compound (referring to the people's such as such as Thridandam US 7875312) and phenyl methyl aminosilane [SiH 3] and the relevant silane aniline (referring to the people's such as such as Xiao EP 2392691) being substituted (NPhMe).
The Si precursor for the CVD containing Si film of another related category is by general formula (R 1r 2n) xsiH 4-xprovide, wherein x between 1 and 4 and R substituting group be H, C1-C6 straight chain, branched chain or ring-type carbochain (referring to the people's such as such as Dussarrat WO2006/097525) independently.
The people such as Hunks disclose many containing Si precursor in US2010/0164057, comprise and have formula R 4-xsiL xsilicon compound, wherein x is the integer with the value of 1-3; R can be selected from H, branched chain and not branched chain C1-C6 alkyl, C3-C8 cycloalkyl and C6-C13 aryl; And L can be selected from isocyanate group, methyl ethyl ketone oxime, trifluoro-acetate, triflate, acyloxy, beta-diketon imines (β-diketiminate), β-bis--imines (β-di-iminate), amidine, guanidine, alkylamino, hydride, alkoxide or manthanoate ligand.The people such as Pinnavaia have advocated a kind of by Acetyl Acetone acid silicon and 1, and 3-diketone silicon (silicon 1,3-diketonate) precursor is prepared the method (US6465387) of the synthetic hypocrystalline organic and inorganic heterozygosis silicon oxide constituent of porous.
Although there are all more options to can be used for the deposition containing Si film, think that unit engineering teacher provides the ability of manufacturing processing procedure requirement and reaching the film with wanted electricity and physical properties that regulates but still constantly find other precursors.
Notation and nomenclature
Run through following specification sheets and claim and use some abbreviation, symbol and term, and comprise:
As used herein, indefinite article " (a/an) " means one (kind) or multiple (kinds).
As used herein, term " independently " in the time of the situation for describing R group, be interpreted as representing described R group not only with respect to identical or different subscript or on other R groups of target select independently, also select independently with respect to any other kind of same R group.For example, at formula MR 1 x(NR 2r 3) (4-x)in (wherein x is 2 or 3), two or three R 1group can but without each other or and R 2or R 3identical.In addition, should be appreciated that, unless other specific statement, in the time being used for different formula, the value of R group is independent of one another.
As used herein, term " alkyl " refers to exclusively contain the saturated functional group of carbon and hydrogen atom.In addition, term " alkyl " refers to straight chain, branched chain or cyclic alkyl.The example of straight chained alkyl includes but not limited to methyl, ethyl, propyl group, butyl etc.The example of branched chain alkyl includes but not limited to the tertiary butyl.The example of cyclic alkyl includes but not limited to cyclopropyl, cyclopentyl, cyclohexyl etc.
As used herein, term " aryl " refers in ring, remove the aromatic compound of a hydrogen atom.As used herein, term " heterocycle " refers to ring compound, and it has the atom of at least two kinds of different elements as the member of its ring.
As used herein, abbreviation " Me " nail base; Abbreviation " Et " refers to ethyl; Abbreviation " Pr " refers to any propyl group (being n-propyl or sec.-propyl); Abbreviation " iPr " refers to sec.-propyl; Abbreviation " Bu " refers to any butyl (normal-butyl, isobutyl-, the tertiary butyl, sec-butyl); Abbreviation " tBu " refers to the tertiary butyl; Abbreviation " sBu " refers to sec-butyl; Abbreviation " iBu " refers to isobutyl-; Abbreviation " Ph " refers to phenyl; Abbreviation " Am " refers to any amyl group (isopentyl, sec.-amyl sec-pentyl secondary amyl, tert-pentyl); Abbreviation " Cy " refers to cyclic alkyl (cyclobutyl, cyclopentyl, cyclohexyl etc.); And abbreviation " R-amd " refers to R-N-C (Me)-N-R amidine ligand, and wherein R is alkyl (for example iPr-amd is iPr-N-C (Me)-N-iPr).
As used herein, acronym " SRO " represents strontium ruthineum oxide film; Acronym " HCDS " represents hexachloro-silane; And acronym " PCDS " represents pentachloro-disilane.
Use the standardized abbreviations of the element of the periodic table of elements herein.Should be appreciated that, can abridge to refer to element (for example Si refers to silicon, and N refers to nitrogen, and O refers to oxygen, and C refers to carbon etc.) with these.
Accompanying drawing summary
In order further to understand character of the present invention and object, should describe in detail with reference to following by reference to the accompanying drawings, wherein similar assembly is specified by identical or similar Ref. No. and wherein:
Fig. 1 is thermogravimetric analysis (TGA) figure, and it shows SiH 3(N iand SiH Pr-amd) 3(N tBu-amd) weight loss per-cent compared with DiPAS (diisopropylaminoethyl silane) under temperature variation; And
Fig. 2 is the figure that shows precursor introducing time contrast sedimentation rate and specific refractory power.
Summary of the invention
Openly there is the organosilane molecule of following formula:
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocyclic radical and R independently of one another 3can be H, C1-C6 alkyl or C3-C20 aryl or heterocyclic radical, amino, alkoxy or halogen;
R 1with R 2and/or R 2with R 3connect to form closed chain;
Organosilane molecule has following formula:
Wherein R 1and R 2can be C1-C6 alkyl independently of one another;
Organosilane molecule is H 3si (N ipr-amd);
Organosilane molecule has following formula:
Wherein R 1, R 2, R 3and R 4can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another;
Organosilane molecule is H 3si (( ipr) N-C (NMe 2)-N ( ipr)-);
Organosilane molecule has following formula:
Wherein R 1, R 2and R 3can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another;
Organosilane molecule is H 3si ((iPr) N-C (OMe)-N (iPr)-);
Organosilane molecule has following formula:
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another; And X can be Cl, Br, I or F; And
Organosilane molecule is H 3si ((iPr) N-C (Cl)-N (iPr)-).
What also openly have following formula forms precursor containing Si film:
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocyclic radical and R independently of one another 3can be H, C1-C6 alkyl, C3-C20 aryl or heterocyclic radical, amino, alkoxy or halogen;
R 1with R 2and/or R 2with R 3connect to form closed chain;
Form precursor containing Si film and there is following formula:
Wherein R 1and R 2can be C1-C6 alkyl independently of one another;
Forming precursor containing Si film is H 3si (N ipr-amd);
Form precursor containing Si film and there is following formula:
Wherein R 1, R 2, R 3and R 4can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another;
Forming precursor containing Si film is H 3si (( ipr) N-C (NMe 2)-N ( ipr)-);
Form precursor containing Si film and there is following formula:
Wherein R 1, R 2and R 3can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another; And
Forming precursor containing Si film is H 3si ((iPr) N-C (OMe)-N (iPr)-);
Form precursor containing Si film and there is following formula:
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another; And X can be Cl, Br, I or F; And
Forming precursor containing Si film is H 3si ((iPr) N-C (Cl)-N (iPr)-).
Also be disclosed in substrate the method for deposition containing Si layer.
Disclosed at least one organosilane precursor is introduced and is wherein mounted with in the reactor of at least one substrate above.Use vapour deposition process that at least a portion organosilane precursor deposition is contained to Si layer to form at least one substrate.Disclosed method can have one or more in following aspect:
In reactor, introduce the steam that comprises at least one the second precursor;
The element of at least one the second precursor is selected from: the 2nd family, the 13rd family, the 14th family, transition metal, lanthanon and combination thereof;
The element of at least one the second precursor is selected from Mg, Ca, Sr, Ba, Zr, Hf, Ti, Nb, Ta, Al, Si, Ge, Y or lanthanon;
In reactor, introduce at least one co-reactant;
Co-reactant is selected from: O 2, O 3, H 2o, H 2o 2, NO, NO 2, carboxylic acid, its free radical and combination thereof;
Co-reactant is the oxygen through plasma treatment;
Co-reactant is ozone;
Be silicon oxide layer containing Si layer;
Co-reactant is selected from: H 2, NH 3, (SiH 3) 3n, hydrosilanes are (as SiH 4, Si 2h 6, Si 3h 8, Si 4h 10, Si 5h 10, Si 6h 12), chlorosilane and chlorine polysilane be (as SiHCl 3, SiH 2cl 2, SiH 3cl, Si 2cl 6, Si 2hCl 5, Si 3cl 8), alkyl silane is (as Me 2siH 2, Et 2siH 2, MeSiH 3, EtSiH 3), hydrazine is (as N 2h 4, MeHNNH 2, MeHNNHMe), organic amine is (as NMeH 2, NEtH 2, NMe 2h, NEt 2h, NMe 3, NEt 3, (SiMe 3) 2nH), pyrazoline, pyridine, containing B molecule (as B 2h 6, 9-boron dicyclo [3,3,1] nonane, trimethyl-boron, triethyl-boron, boron azine (borazine)), metal alkylide (as trimethyl aluminium, triethyl aluminum, zinc methide, zinc ethyl), its free radical material and composition thereof.
Co-reactant is selected from: H 2, NH 3, SiH 4, Si 2h 6, Si 3h 8, SiH 2me 2, SiH 2et 2, N (SiH 3) 3, its hydroperoxyl radical and composition thereof;
Co-reactant is through plasma treatment;
Co-reactant is through remote plasma processing;
Co-reactant is without plasma treatment;
Co-reactant is H 2;
Co-reactant is NH 3;
Co-reactant is HCDS;
Co-reactant is PCDS;
Co-reactant is tetrachloro silicane;
Co-reactant is trichlorosilane;
Co-reactant is chlordene ring six silane;
Vapour deposition process is chemical Vapor deposition process;
Vapour deposition process is ald (ALD) method;
Vapour deposition process is space ALD method;
Silicon-containing layer is Si;
Silicon-containing layer is SiO 2;
Silicon-containing layer is SiN;
Silicon-containing layer is SiON;
Silicon-containing layer is SiCN; And
Silicon-containing layer is SiCOH.
Embodiment
Disclose containing Si film and formed precursor, its synthetic method and use it to use the method for vapour deposition process depositing silicon-containing films for the manufacture of semi-conductor, photovoltaic devices, LCD-TFT, plate device, refractory materials or aeronautical material.
Disclosed organosilane precursor has following formula:
Amidine
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocyclic radical and R independently of one another 3can be H, C1-C6 alkyl, C3-C20 aryl or heterocyclic radical, amino, alkoxy or halogen.R 1and R 2and/or R 2and R 3can connect to form closed chain.
As illustrated in this formula, nitrogen-atoms is binding on Siliciumatom, thereby produces pentacoordinate Si (IV) center.Carbon atom in the main chain of bidentate single anion ligand is sp 2hydridization, thus non-localized electric charge in ligand, produced.Nitrogen and carbon atom can replace through H, C1-C6 alkyl, aryl or heterocyclic radical independently of one another.
Disclosed organosilane precursor may be than other R due to the super coordination at Siliciumatom place 4-xsiL xprecursor has more reactivity.In other words, although Siliciumatom is+IV that three hydrogen bonds and single anion chelating ligand and Siliciumatom form 5 keys altogether.
Those skilled in the art will recognize that and use alkyl, aryl or the heterocyclic radical (being H, C1 or C2) in hydrogen or any R group with less carbon atom, compared with thering is the molecule of the alkyl, aryl or the heterocyclic radical that contain more carbon (being C4+), generation is had to more high-volatile molecule.Because the nitrogen content of its two nitrogen-atoms in-N-C-N-ligand increases, these molecules can be used for producing the silicon-containing film that also contains nitrogen, as SiN, SiCN, SiON, MSiN or MSiON, wherein M is as the element of Hf, Zr, Ti, Nb, Ta or Ge, or for regulating the amount of nitrogen of they's film.
Work as R 3during for Me, gained precursor is the compound that contains amidine with following formula:
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocyclic radical independently of one another.Preferably, R1 and R2 are respectively C1-C6 alkyl independently.
Amidine precursor can synthesize as follows: by by SiXH 3(wherein X is Cl, Br, I or trifluoromethanesulfonic acid root (SO 3cF 3 -)) hydrocarbon solution and pure ligand compound (as Li[R 1nC (R 2) NR 3] or Li (amd)) or its hydrocarbon solution under nitrogen atmosphere, combine, the outlet and the oily bubbler that mix flask are connected to suppress air and moisture backflow.
The second route of synthesis that obtains disclosed amidine precursor is by make protonated ligand (R under inert atmosphere 1n=C (R 2)-NRH 3) and pure dialkyl amino base silane [SiH 3(NR 2)] or its hydrocarbon solution reaction.
Or disclosed amidine precursor can synthesize as follows: pass through SiH ncl 4-nwith the ligand compound of single equivalent (be Li[R 1nC (R 2) NR 3] or Li (amd)) reaction, use subsequently selected metal hydride (as LAH (lithium aluminium hydride)) reduction.
In all three route of synthesis, can at room temperature stir gained solution and spend the night.The exemplary hydrocarbon solution that is suitable for these synthetic methods comprises ether, pentane, hexane or toluene.Filter gained suspension and distillation gained solution to remove solvent.Respectively by distilling or the purifying gained liquid or solid that distils.Except ligand compound Li (amd), all parent materials all can buied on the market.Ligand compound can be by (being R by the hydrocarbon solution of organic metal salt (being lithium alkylide) with suitable carbodiimide 1n=C=NR 3) hydrocarbon solution synthesize.Other synthetic details are provided in embodiment.
Exemplary amidine precursor comprises:
Preferably, amidine precursor is SiH 3(N ipr-amd).
Work as R 3for amino (is NR 3r 4) time, gained precursor is the compound that contains guanidine with following formula:
Guanidine
Wherein R 1, R 2, R 3and R 4can be H, C1-C6 alkyl, C3-C20 aryl or heterocycle independently of one another.Due to it, nitrogen content increases compared with other molecules time, and these molecules can be used for producing the silicon-containing film (as SiN or SiON) that also contains nitrogen, or for regulating the amount of nitrogen of the film that contains SiN or SiON.
Guanidine precursor can synthesize as follows: by by SiXH 3(wherein X is Cl, Br, I or trifluoromethanesulfonic acid root (SO 3cF 3 -)) hydrocarbon solution and pure ligand compound (as Li[R 1nC (NR 3r 4) NR 2] (or Li (gnd))) or its hydrocarbon solution under nitrogen atmosphere, combine, the outlet and the oily bubbler that mix flask are connected to suppress air and moisture backflow.
The second route of synthesis that obtains disclosed guanidine precursor is by make protonated ligand (R under inert atmosphere 1n=C (NR 3r 4)-NR 2h) with pure dialkyl amino base silane [SiH 3(NR 2)] or its hydrocarbon solution reaction.
Or disclosed guanidine precursor can synthesize as follows: pass through SiH ncl 4-nwith the ligand compound of single equivalent (be Li[R 1nC (NR 3r 4) NR 2] or Li (gnd)) reaction, use subsequently selected metal hydride (as LAH (lithium aluminium hydride)) reduction.
In all three route of synthesis, can at room temperature stir gained solution and spend the night.The exemplary hydrocarbon solution that is suitable for these synthetic methods comprises ether, pentane, hexane or toluene.Filter gained suspension and distillation gained solution to remove solvent.Respectively by distilling or the purifying gained liquid or solid that distils.Except ligand compound Li (gnd), all parent materials all can buied on the market.Ligand compound can be by (being Lithamide-Li (NR by organic metal salt 3r 4)) hydrocarbon solution (be R with suitable carbodiimide 1n=C=NR 2) hydrocarbon solution synthesize.
Exemplary guanidine precursor comprises:
Preferably, guanidine precursor is H 3si (( ipr) N-C (NMe 2)-N ( ipr)-).
Work as R 3for alkoxyl group (is OR 3) time, gained precursor is the compound that contains isourea with following formula:
Isourea
Wherein R 1, R 2and R 3can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another.
Due to it, oxygen level increases compared with other molecules time, and these molecules also can be used for producing silicon-containing film containing aerobic (as SiO 2or SiON), or contain SiO for regulating 2or the amount of oxygen in the film of SiON.
Isourea precursor can synthesize as follows: by by SiXH 3(wherein X is Cl, Br, I or trifluoromethanesulfonic acid root (SO 3cF 3-)) hydrocarbon solution and pure ligand compound (as Li[R 1nC (OR 3) NR 2] (or Li (iso))) or its hydrocarbon solution under nitrogen atmosphere, combine, the outlet and the oily bubbler that mix flask are connected to suppress air and moisture backflow.
The second route of synthesis that obtains disclosed isourea precursor is by make protonated ligand (R under inert atmosphere 1n=C (OR 3)-NR 2h) with pure dialkyl amino base silane [SiH 3(NR 2)] or its hydrocarbon solution reaction.
Or disclosed isourea precursor can synthesize as follows: pass through SiH ncl 4-nwith the ligand compound of single equivalent (be Li[R 1nC (OR 3) NR 2] or Li (iso)) reaction, use subsequently selected metal hydride (as LAH (lithium aluminium hydride)) reduction.
In all three route of synthesis, can at room temperature stir gained solution and spend the night.The exemplary hydrocarbon solution that is suitable for these synthetic methods comprises ether, pentane, hexane or toluene.Filter gained suspension and distillation gained solution to remove solvent.Respectively by distilling or the purifying gained liquid or solid that distils.Except ligand compound Li (iso), all parent materials all can buied on the market.Ligand compound can be by (being alkanol lithium-Li (OR by organic metal salt 3)) hydrocarbon solution (be R with suitable carbodiimide 1n=C=NR 2) hydrocarbon solution synthesize.
Exemplary isourea precursor comprises:
Preferably, isourea precursor is H 3si ((iPr) N-C (OMe)-N (iPr)-).
Work as R 3during for halogen (being X), gained precursor is the compound that contains α-halogen amidine with following formula:
α-halogen amidine
Wherein R 1and R 2can be that H, C1-C6 alkyl or C3-C20 aryl or heterocycle and X can be Cl, Br, I or F independently of one another.Halogen atom can improve the conformality of the ald of non-crystalline silicon.
α-halogen amidine precursor can synthesize as follows: by combining through disubstituted urea derivatives R 1hN-(C=O)-NHR 2hydrocarbon solution and O=CX 2hydrocarbon solution, as described in the people such as Neubauer (Chemische Berichte, 1964,97 (5), 1232-1245).Add the hydrocarbon solution of suitable alkali (as hexamethyldisilane potassium amide) of a molar equivalent to reaction mixture, and filter gained suspension to remove metal-salt by product.Gained solution can with SiRH 3reaction, wherein R is phenyl, tolyl or other suitable aryl substituents.Gained mixture can be by fractionation purifying.The exemplary hydrocarbon solution that is suitable for these synthetic methods comprises ether, pentane, hexane or toluene.All parent materials all can buied on the market.
Exemplary α-halogen amidine precursor comprises:
Preferably, α-halogen amidine is H 3si ((iPr) N-C (Cl)-N (iPr)-).
Also openly use disclosed organosilane precursor to carry out the method for vapour deposition process.Disclosed method provides the purposes of organic silane precursor for depositing silicon-containing films.Disclosed method is applicable to manufacturing semi-conductor, photovoltaic devices, LCD-TFT or plate device.The method comprises: substrate is provided; At least one the steam comprising in disclosed organosilane precursor is provided; And make steam and substrate contact (and typically steam being directed to substrate) to form silicon-containing layer at least one surface of substrate.
Disclosed method also can be used vapour deposition process in substrate, to form containing double-metal layer and deposition SiMO in more specific words xfilm, wherein x be 4 and M be Ta, Hf, Nb, Mg, Al, Sr, Y, Ba, Ca, As, Sb, Bi, Sn, Pb, Co, lanthanon (as Er) or its combination.Disclosed method is applicable to manufacturing semi-conductor, photovoltaic devices, LCD-TFT or plate device.The method comprises: substrate is provided; Provide comprise in disclosed organosilane precursor at least one steam and make steam and substrate contact (and typically steam being directed to substrate) to form containing bimetallic layer at least one surface of substrate.As O 3, O 2, H 2o, NO, H 2o 2, acetic acid, formalin, trioxymethylene, its oxyradical and combination thereof but preferred O 3or through the O of plasma treatment 2oxygen source also can provide together with steam.
Disclosed organosilane precursor can be used for any deposition silicon-containing film that uses those skilled in the art known.The example that is applicable to deposition method includes but not limited to known chemical vapour deposition (CVD), low-pressure chemical vapor deposition (LPCVD), ald (ALD), pulsed chemical vapour deposition (P-CVD), hot ALD, hot CVD, plasma enhanced ald (PE-ALD), plasma enhanced chemical vapor deposition (PE-CVD), space ALD or its combination.Preferably, deposition method is ALD, space ALD or PE-ALD.
Organosilane precursor vapor is introduced in the reaction chamber that contains at least one substrate.Temperature and pressure in reaction chamber and the temperature of substrate remain on and are suitable at least a portion organosilane precursor gas phase to be deposited under suprabasil condition.In other words, in vaporized precursor is introduced to chamber after, the condition in chamber makes at least a portion vaporized precursor be deposited in substrate to form silicon-containing film.Co-reactant also can be used for helping to form containing Si layer.
Reaction chamber can be any closed region or the chamber that in device, carry out deposition method, as but be not limited to the sedimentary system of parallel plate type reactor, cold-wall type reactor, hot wall type reactor, single-wafer reactor, many wafer reactor or other these types.All these exemplary reaction chambers all can serve as ALD reaction chamber.Reaction chamber can maintain approximately 0.5 millitorr to the pressure within the scope of approximately 20 holders.In addition, the temperature in reaction chamber can be within the scope of approximately 20 DEG C to approximately 600 DEG C.Those skilled in the art will recognize that can only optimize temperature via experiment is wanted result to reach.
Can control temperature of reactor by the temperature of the temperature of control substrate holder or control reactor wall.Be that this area is known for the device that heats substrate.Reactor wall is heated to the temperature that is enough to obtain under sufficient growth velocity and there is the film of wanting of wanted physical condition and composition.The non-limiting exemplary temperature range that reactor wall can be heated to comprises approximately 20 DEG C to approximately 600 DEG C.In the time using plasma deposition processes, depositing temperature can be within the scope of approximately 20 DEG C to approximately 550 DEG C.Or in the time carrying out hot processing procedure, depositing temperature can be within the scope of approximately 300 DEG C to approximately 600 DEG C.
Or, substrate can be heated to the temperature that is enough to obtain under sufficient growth velocity and there is the silicon-containing film of wanting of wanted physical condition and composition.The non-limiting exemplary temperature range that substrate can be heated to comprises 150 DEG C to 600 DEG C.Preferably, base reservoir temperature keeps below or equals 500 DEG C.
The type of the substrate of depositing silicon-containing films will be looked to the end-use of expection and difference above.In some specific embodiments, substrate for example can be, by hydrogenated carbon (CH x, wherein x is greater than zero) and the patterning photoresistance film made.In some specific embodiments, the oxide compound that is used as dielectric materials in the optional comfortable MIM of substrate, DRAM or FeRam technology is (for example, based on ZrO 2material, based on HfO 2material, based on TiO 2material, the material based on rare earth oxide, the material based on ternary oxide (ternary oxide) etc.) or be selected from the film based on nitride (for example TaN) as the oxygen barrier between copper and low k layer.Can manufacture semi-conductor, photovoltaic devices, LCD-TFT or board device with other substrates.The example of this type of substrate includes but not limited to solid substrate, as the substrate that contains metal nitride (for example TaN, TiN, WN, TaCN, TiCN, TaSiN and TiSiN); Isolator (for example SiO 2, Si 3n 4, SiON, HfO 2, Ta 2o 5, ZrO 2, TiO 2, Al 2o 3and barium strontium); Or comprise other substrates of the multiple combination of these materials.The actual base using is also determined by used specific precursor specific embodiments.But in many cases,, the preferred substrate using will be selected from hydrogenated carbon, TiN, SRO, Ru and the substrate of Si type, as polysilicon or silicon metal substrate.
Disclosed organosilane precursor can pure form or with applicable solvent (as toluene, ethylbenzene, dimethylbenzene, sym-trimethylbenzene, decane, dodecane, octane, hexane, pentane, tertiary amine, acetone, tetrahydrofuran (THF), ethanol, ethyl methyl ketone, Isosorbide-5-Nitrae-bis- alkane or other solvents) blend form supply.Disclosed precursor can be present in solvent by different concns.For example, gained concentration can be at about 0.05M to about 2M.
Organosilane precursor pure or blending is introduced in reactor with steam form by known members (as pipeline and/or under meter).Can be by making precursor solution pure or blending vaporize to produce the precursor that is steam form via known pervaporation step (as direct boiling, distillation, by bubbling or by using sublimer (disclosed sublimer in case WO2009/087609 as open in the people's such as Xu PCT)).Precursor pure or blending can liquid state be filled in vaporizer, and in this vaporizer, it is introduced in reactor subsequently through vaporization.Or, can be by carrier gas being passed in the container that contains precursor or by making carrier gas bubbling make precursor vaporization pure or blending to precursor.Carrier gas can include but not limited to Ar, He or N 2and composition thereof.With the carrier gas bubbling also removable any dissolved oxygen being present in precursor solution pure or blending.Then, carrier gas and precursor are introduced in reactor with steam form.
If desired, container can be heated to the temperature that allows organosilane precursor to be its liquid phase and there is sufficient vapour pressure.At the temperature of container within the scope of for example can maintaining 0-150 DEG C.Those skilled in the art recognize and can regulate in a known way the temperature of container to control the amount of the organosilane precursor of vaporizing.
Except disclosed precursor, reactant gases (being co-reactant) also can be introduced in reactor.Reactant gases can be oxygenant, the one as with lower: O 2; O 3; H 2o; H 2o 2; Oxygen radical, as O or OH; NO; NO 2; Carboxylic acid, as formic acid, acetic acid, propionic acid; NO, NO 2or the free radical material of carboxylic acid; Trioxymethylene; And composition thereof.Preferably, oxygenant is selected from: O 2, O 3, H 2o, H 2o 2, its oxygen radical (as O or OH) and composition thereof.Preferably, in the time carrying out ALD processing procedure, co-reactant is through the oxygen of plasma treatment, ozone or its combination.In the time using oxidizing gas, gained silicon-containing film also will be containing aerobic.
Or reactant gases can be reductive agent, the one as with lower: H 2, NH 3, (SiH 3) 3n, hydrosilanes are (as SiH 4, Si 2h 6, Si 3h 8, Si 4h 10, Si 5h 10, Si 6h 12), chlorosilane and chlorine polysilane be (as SiHCl 3, SiH 2cl 2, SiH 3cl, Si 2cl 6, Si 2hCl 5, Si 3cl 8), alkyl silane is (as (CH 3) 2siH 2, (C 2h 5) 2siH 2, (CH 3) SiH 3, (C 2h 5) SiH 3), hydrazine is (as N 2h 4, MeHNNH 2, MeHNNHMe), organic amine is (as N (CH 3) H 2, N (C 2h 5) H 2, N (CH 3) 2h, N (C 2h 5) 2h, N (CH 3) 3, N (C 2h 5) 3, (SiMe 3) 2nH), pyrazoline, pyridine, containing B molecule (as B 2h 6, 9-boron dicyclo [3,3,1] nonane, trimethyl-boron, triethyl-boron, boron azine), metal alkylide (as trimethyl aluminium, triethyl aluminum, zinc methide, zinc ethyl), its free radical material and composition thereof.Preferably, reductive agent is H 2, NH 3, SiH 4, Si 2h 6, Si 3h 8, SiH 2me 2, SiH 2et 2, N (SiH 3) 3, its hydroperoxyl radical or its mixture.In the time using reductive agent, gained silicon-containing film can be pure Si.
Reactant gases can be through plasma treatment, to make reactant gases resolve into its radical form.N when through plasma treatment 2also can be used as reductive agent.For example, can produce power at about 50W to about 500W, preferred about 100W to the plasma within the scope of about 200W.Plasma can produce or be present in reactor self.Or plasma can be conventionally for example, in moving apart the position of reactor, in the plasma based of long range positioning.Those skilled in the art will expect being suitable for method and the device of this plasma treatment.
Disclosed organosilane precursor also can use together with halogenated silanes or poly-halogenated silanes (as hexachloro-silane, pentachloro-disilane or tetrachloro disilane) and one or more co-reactant gases, to form SiN or SiCN film, disclosed in No. WO2011/123792nd, case as open in PCT, the full content of the disclosure case is incorporated herein for reference.
When wanted silicon-containing film also contain another element (as but be not limited to Ta, Hf, Nb, Mg, Al, Sr, Y, Ba, Ca, As, Sb, Bi, Sn, Pb, Co, lanthanon (as Er) or its combination) time, co-reactant can comprise containing metal precursor, it is selected from but is not limited to metal alkyl, as Ln (RCp) 3or Co (RCp) 2; Metal amine, as (NtBu) (NMe of Nb (Cp) 2) 3; And any combination.
Organosilane precursor and one or more co-reactants be (chemical vapour deposition), (ald) or introduce in reaction chambers with other array configurations in succession simultaneously.For example, organosilane precursor can be introduced and two kinds of other metal sources can be introduced together [improved ald] in independent pulse in pulsatile once.Or reaction chamber may contain co-reactant before introducing organosilane precursor.Can make co-reactant by being positioned the long-range plasma based of reaction chamber, and resolve into free radical.Or organosilane precursor can be introduced in reaction chamber continuously, and other metal sources are introduced (pulsed chemical vapour deposition) by pulse.In each embodiment, can after pulse, purge or excessive component that evacuation step is introduced to remove.In each embodiment, the sustainable about 0.01s of pulse is to about 10s, or about 0.3s is to about 3s, or about 0.5s is to the time within the scope of about 2s.In another replacement scheme, organosilane precursor and one or more co-reactants can spray from showerhead simultaneously, the pedestal of the some wafers of fixing rotation (space ALD) under this showerhead.
In a non-limiting exemplary ald type processing procedure, the gas phase of organosilane precursor is introduced in reaction chamber, itself and applicable substrate contact in this reaction chamber.Then, can by purge and/or the reaction chamber of finding time from removing excessive organosilane precursor in reaction chamber.Oxygen source is introduced in reaction chamber, in this reaction chamber its with absorbed organosilane precursor to react from ways to restrain.By purge and/or the reaction chamber autoreaction chamber of finding time in remove any excessive oxygen source.If the film of wanting is silicon oxide film, this two steps processing procedure can provide wanted film thickness maybe can repeat until obtained the film with essential thickness.
Or, (be SiMO if the film of wanting is silicon metal oxide film xwherein x can be 4 and M be Ta, Hf, Nb, Mg, Al, Sr, Y, Ba, Ca, As, Sb, Bi, Sn, Pb, Co, lanthanon (as Er) or its combination), can be by the second steam introducing reaction chamber of containing metal precursor above two step processing procedures after.Containing metal precursor is selected the character of the silicon metal oxide film based on deposited.After introducing in reaction chamber, containing metal precursor and substrate contact.By purge and/or the reaction chamber autoreaction chamber of finding time in remove any excessive containing metal precursor.Again, oxygen source can be introduced in reaction chamber with containing metal precursors reaction.In reaction chamber autoreaction chamber, remove excessive oxygen source by purging and/or finding time.If reached wanted film thickness, processing procedure can stop.But, if desired compared with thick film, can repeat whole four step process.To form and the film of thickness by organic silane precursor, containing metal precursor and oxygen source being alternately provided, can depositing to have.
In addition, by changing pulse number, can obtain the film with wanted stoichiometry M:Si ratio.For example, by carrying out the pulse of an organosilane precursor and the pulse of a containing metal precursor, and the pulse of carrying out oxygen source after each pulse can obtain SiMO 2film.But, those skilled in the art will recognize that for obtain the required pulse number of the film of wanting may be not equal to the stoichiometric ratio of gained film.
In another replacement scheme, can use disclosed compound and there is formula Si via ALD or improved ALD processing procedure ah 2a+2-bx b(wherein X is F, Cl, Br or I; A=1 to 6; And b=1 is to (2a+2)) halogenated silanes compound; Or there is formula-Si ch 2c-dx d-(wherein X is F, Cl, Br or I; C=3-8; And d=1 to 2c) ring-type halogenated silanes Compound deposition Si or fine and close SiCN film.Preferably, halogenated silanes compound is trichlorosilane, hexachloro-silane (HCDS), pentachloro-disilane (PCDS), tetrachloro disilane or chlordene ring six silane.Those skilled in the art will recognize that when essential when compared with low deposition temperature the Cl in these compounds can replace through Br or I, this lower bond energy owing to Si-X key (is Si-Cl=456kJ/mol; Si-Br=343kJ/mol; Si-I=339kJ/mol).If desired, deposition can further be used containing N reactant, as NH 3.The visual desired final film concentration of steam of disclosed precursor and halogenated silanes compound and in succession or simultaneously introduce reactor.Selected precursor injection order is determined the film composition based on institute's syllabus.Can repeat precursor and introduce step until settled layer is reached applicable thickness.Those skilled in the art will recognize that guided bone pulse (introductory pulse) can be simultaneously in the time of usage space ALD device.Described in No. WO2011/123792nd, case as open in PCT, can change precursor introducing order and can have or not exist NH 3under co-reactant, carry out deposition, to regulate the amount of carbon and nitrogen in SiCN film.
The silicon-containing film being produced by the processing procedure above discussed can comprise Si, SiN, SiON, SiCN, SiCOH or MSiO x, wherein M is as the element of Hf, Zr, Ti, Nb, Ta or Ge, and x can be 4, certainly depending on the oxidation state of M.Those skilled in the art will recognize that by the suitable organosilane precursor of careful selection and co-reactant, can obtain wanted film composition.
Acquisition is wanted after film thickness, can be further processed film, as thermal annealing, furnace annealing, rapid thermal annealing, UV or electrocuring and/or plasma gas exposure.Those skilled in the art are conceivable for carrying out the system and method for these additional processing steps.For example, silicon-containing film is exposed to the temperature within the scope of approximately 200 DEG C to approximately 1000 DEG C, the time within the scope of lasting approximately 0.1 second to approximately 7200 seconds under can be at inert atmosphere, containing H atmosphere, containing N atmosphere, containing O atmosphere or its combination.Most preferably, temperature is 400 DEG C, containing continuing 3600 seconds under H atmosphere.Gained film can contain less impurity, and therefore can have improved performance characteristics.Can in the same reaction chamber of carrying out deposition manufacture process, carry out annealing steps.Or, can in autoreaction chamber, remove substrate, and carry out annealing/hurried annealing process in self-contained system.Found in above post-treating method any, especially thermal annealing can effectively reduce carbon and the polluted by nitrogen of silicon-containing film.
Embodiment
Provide following non-limiting example to further illustrate specific embodiment of the invention scheme.But these embodiment are also not intended to comprise all and are not intended to limit invention category as herein described.
embodiment 1
SiH 3(N isynthesizing Pr-amd): under agitation, the diethyl ether solution of lithium methide (91mL, 1.6M, 0.146mol) is slowly added into N, in-40 DEG C of solution of N'-di-isopropyl carbodiimide (22.5mL, 0.145mol) in ether (150mL).After having added, make the colourless suspension of gained be warming up to room temperature and stir three hours to form colourless solution.In the independent flask that is equipped with-78 DEG C of (dry ice/acetone) condensers, pack ether (100mL) into and be cooled to-78 DEG C.Under agitation, monochlorosilane (13.2g, 0.198mol) is slowly condensed in the second flask, slowly adds subsequently the amidino groups lithium solution from first step.Original observed being fuming to a certain extent, forms colourless precipitation subsequently.Complete after interpolation, under vigorous stirring is spent the night, make suspension slowly reach to room temperature.Medium glass powder filtering suspension liquid through containing Celite pad and under atmospheric pressure use Wei Geluo tubing string (Vigreux column) distillation gained colourless solution to remove solvent.Change and receive flask and cooling in-78 DEG C of baths, under 25-28 DEG C/200-300 millitorr, distillation obtains being the required product of colourless liquid shape.Output: 7.9g (31.6%).Fig. 1 is the TGA figure that shows this precursor weight loss per-cent under temperature variation compared with DiPAS. 29Si?NMR(80MHz,C 6D 6,25℃)δ(ppm)＝-87.7； 1H?NMR(400MHz,C 6D 6,25℃)δ(ppm)＝4.73(s,3H,SiH 3),3.38(sept.,2H, 1J H-H＝8.0Hz,NCH(CH 3) 2),1.40(s,3H,CCH 3),1.12(d,12H, 1J H-H＝8.0Hz,NCH(CH 3) 2)。
embodiment 2
SiH 3(N tsynthesizing Bu-amd): pack ether (100mL) into and be cooled to-78 DEG C in the flask that is equipped with-78 DEG C of (dry ice/acetone) condensers.Under agitation, monochlorosilane (8.9g, 0.134mol) is slowly condensed in flask.In the second flask, the diethyl ether solution of lithium methide (101mL, 1.6M, 0.162mol) is slowly added into N, in-40 DEG C of solution of N'-bis--tertiary butyl carbodiimide (25g, 0.162mol) in ether (100mL).After having added, make the colourless suspension of gained amidino groups lithium be warming up to room temperature and stir one hour to form colourless solution.Gained Li-amd solution is cooled to 0 DEG C and be added in-78 DEG C of solution of monochlorosilane (MCS) in ether by sleeve pipe.Original observed being fuming to a certain extent, forms colourless precipitation subsequently.Complete after interpolation, under vigorous stirring, suspension is reached to room temperature.
Stop stirring, and make solid settlement with after filter through the medium glass powder with bed of diatomaceous earth.Gained colourless solution is transferred in the flask that contains dry Amberlyst A21 resin (5g), slightly stirs and make it at room temperature leave standstill 14 hours.Then, filtering solution and under atmospheric pressure use short distance tubing string to distill to remove solvent and high volatile matter, thus obtain high viscosity light yellow liquid.Change and receive flask and be cooled to-78 DEG C, under 55-61 DEG C/100 millitorrs, distillation obtains being the required product of colourless liquid shape, and it at room temperature leaves standstill slowly crystallization afterwards.Output: 14.5g (54.1%).MP＝36℃, 29Si?NMR(80MHz,C 6D 6,25℃)δ(ppm)＝-117.5； 1H?NMR(400MHz,C 6D 6,25℃)δ(ppm)＝5.05(s,3H,SiH 3),1.79(s,3H,CCH 3),1.25(s,9H,NC(CH 3) 3)。
embodiment 3
SiH 3(N ipr-amd) ALD: the SiH that uses preparation in embodiment 1 3(N ipr-amd) carry out ALD test, by this SiH 3(N ipr-amd) be placed in the container under room temperature.Use typical ALD condition, as used ozone under the reactor pressure being fixed on approximately 0.5 holder.As shown in Figure 2, at 275 DEG C, on pure silicon wafer, assess the ALD characteristic under completely surperficial saturated and response situation.Those skilled in the art will recognize that different depositing devices can represent surface in the different precursor introducing time saturated.Specific refractory power is SiO 2characteristic (the pure SiO of film 2specific refractory power be 1.46).Changed the impurity in the variations in refractive index instruction film causing by the precursor introducing time.
Should be appreciated that, in the principle of the invention and category of being explained in as appended claim, those skilled in the art can be to having described and having illustrated to explain that details, material, step and the component configuration of character of the present invention make many other changes herein.Therefore, the present invention be not intended to be limited to the specific specific embodiments in above provided embodiment and/or accompanying drawing.

Claims (14)

1. form a precursor containing Si film, it has following formula:
Wherein R 1and R 2can be H, C1-C6 alkyl or C3-C20 aryl or heterocyclic radical and R independently of one another 3can be H, C1-C6 alkyl, C3-C20 aryl or heterocyclic radical, amino, alkoxy or halogen.
2. form precursor according to the Si film that contains of claim 1, it has following formula:
Wherein R 1and R 2can be C1-C6 alkyl independently of one another.
3. form precursor according to the Si film that contains of claim 2, wherein molecule is SiH 3(N ipr-amd).
4. form precursor according to the Si film that contains of claim 1, it has following formula:
Wherein R 1, R 2, R 3and R 4can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another.
5. form precursor according to the Si film that contains of claim 1, it has following formula:
Wherein R 1, R 2and R 3can be H, C1-C6 alkyl or C3-C20 aryl or heterocycle independently of one another.
6. form precursor according to the Si film that contains of claim 1, it has following formula:
Wherein R 1and R 2can be that H, C1-C6 alkyl or C3-C20 aryl or heterocycle and X can be Cl, Br, I or F independently of one another.
7. in substrate, deposition is containing a method for Si layer, and described method comprises:
At least one organosilane precursor according to any one in claim 1-6 is introduced and is wherein mounted with in the reactor of at least one substrate;
Use vapour deposition process that at least a portion organosilane precursor deposition is contained to Si layer to form at least one substrate.
8. according to the method for claim 7, it further comprises in reactor introduces at least one co-reactant.
9. method according to Claim 8, wherein co-reactant is selected from: O 2, O 3, H 2o, H 2o 2, NO, NO 2, carboxylic acid, its free radical and combination thereof, preferably through oxygen or the ozone of plasma treatment.
10. method according to Claim 8, wherein co-reactant is selected from: H 2, NH 3, (SiH 3) 3n, hydrosilanes are (as SiH 4, Si 2h 6, Si 3h 8, Si 4h 10, Si 5h 10, Si 6h 12), chlorosilane and chlorine polysilane be (as SiHCl 3, SiH 2cl 2, SiH 3cl, Si 2cl 6, Si 2hCl 5, Si 3cl 8), alkyl silane is (as Me 2siH 2, Et 2siH 2, MeSiH 3, EtSiH 3), hydrazine is (as N 2h 4, MeHNNH 2, MeHNNHMe), organic amine is (as NMeH 2, NEtH 2, NMe 2h, NEt 2h, NMe 3, NEt 3, (SiMe 3) 2nH), pyrazoline, pyridine, containing B molecule (as B 2h 6, 9-boron dicyclo [3,3,1] nonane, trimethyl-boron, triethyl-boron, boron azine), metal alkylide (as trimethyl aluminium, triethyl aluminum, zinc methide, zinc ethyl), its free radical material and composition thereof.
11. according to the method for claim 10, and wherein co-reactant is selected from: H 2, NH 3, SiH 4, Si 2h 6, Si 3h 8, SiH 2me 2, SiH 2et 2, N (SiH 3) 3, its hydroperoxyl radical and composition thereof.
12. according to the method for claim 10, and wherein co-reactant is selected from: SiHCl 3, Si 2cl 6, Si 2hCl 5, Si 2h 2cl 4and ring-Si 6h 6cl 6.
13. according to the method for claim 7, and wherein vapour deposition process is chemical Vapor deposition process.
14. according to the method for claim 7, and wherein vapour deposition process is atomic layer deposition method.
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